CN101974326B - Method for preparing novel fluorescent silica nanospheres - Google Patents
Method for preparing novel fluorescent silica nanospheres Download PDFInfo
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- CN101974326B CN101974326B CN 201010291074 CN201010291074A CN101974326B CN 101974326 B CN101974326 B CN 101974326B CN 201010291074 CN201010291074 CN 201010291074 CN 201010291074 A CN201010291074 A CN 201010291074A CN 101974326 B CN101974326 B CN 101974326B
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Abstract
The invention relates to a method for preparing fluorescent silica nanospheres and belongs to the technical field of inorganic chemistry and material synthesis. The main process of the method of the invention mainly comprises: (1) according to the prior art, calcining a certain amount of ethylene diamine tetraacetic acid (EDTA-2Na) at 250 to 400 DEG C in the presence of N2 in a tube furnace to obtain fluorescent carbon quantum dots; (2) mixing the fluorescent carbon quantum dots, deionized water, octadecylamine and methylbenzene, reacting at 160 to 180 DEG C for 12 hours, centrifuging, separating, collecting supernate and drying to obtain octadecylamine-modified fluorescent carbon quantum dots; and (3) mixing the octadecylamine-modified fluorescent carbon quantum dots with water, ethanol, ammonia water and ethyl orthosilicate, reacting at 40 DEG C for 1 to 12 hours, adding the ethyl orthosilicate and the hexadecy ltrimethyl ammonium bromide, reacting for 1 to 12 hours, washing with ethanol, centrifuging, drying and calcining at 300 DEG C for 3 hours and thus obtaining the fluorescent silica nanospheres.
Description
Technical field
The present invention relates to a kind of preparation method of fluorescent silicon dioxide nanospheres, exactly, relate to a kind of composite manufacture method of coated with silica fluorescent carbon quantum dot, belong to inorganic chemistry and field of material synthesis technology.
Background technology
Over past ten years, semiconductor-quantum-point (Quantum dot) is because having the adjustable fluorescent emission of size, narrow and symmetrical emmission spectrum, wide and continuous absorption spectrum, fabulous a series of uniquenesses such as light stability optical, cause that people pay close attention to widely, be expected to replace the organic dye probe to become the good fluorescent probe of a new generation, and will play the part of important role in the probe mark detection technique in future and correlative study.Yet fluorescence semiconductor quantum dots mainly is made of II/VI family and III/group Ⅴ element, and usually take CdSe as core, CdS or ZnS are the core-shell nanometer body of shell, during as bioprobe, no matter is used in body or in vitro tests, heavy metal Cd at it
2+Release larger to the damage of cell, particularly aspect the living body biological cell marking; Add that to the potential destruction of environment, these have all seriously limited the biologic applications of semiconductor-quantum-point.
As far as we know, carbon material is a kind of have good biological security, hypotoxicity, environment-friendly type quality matetrial.Material take carbon nanotube as representative has been widely used in the researchs such as biological medicine carrying and biosensor, experimental results show that carbon nanotube toxicity is low, and biological safety is good.The preparation of fluorescent carbon quantum dot recently causes the great interest of people, fluorescent carbon quantum dot has that low toxicity is even nontoxic, fluorescence is extremely stable, the emission wavelength wide region is adjustable, with low cost, be easy to realize the characteristics such as physiologically acceptable, be the novel fluorescent nano material of a class.Compare with containing the unsettled semiconductor-quantum-point fluorescent material of toxic metal ion and fluorescence, fluorescent carbon quantum dot is applied to the more aobvious advantage of biomedical sector as fluorescent probe.
Silica nanosphere because having the advantages such as Stability Analysis of Structures, nontoxicity and biocompatibility, is one of drug molecule carrier ideal material.Wherein, Vallet-Regi etc. as drugs, have carried out the research of this respect with the anti-inflammation analgesic Ibuprofen BP/EP the earliest, find that MCM-41 can absorb and discharge the organic drug molecule, and when material was immersed in the body fluid of simulation, medicine was slowly released.People slowly find afterwards, the mesoporous material as main body is carried out carrying out suitable cutting on the modification of suitable organic functional group or pattern be conducive to drug conveying.Fluorescently-labeled SiO
2Nanometer ball is owing to being easy to observation, and the Chang Zuowei model is used to study the interaction of nanometer ball and cell and tissue, thereby mechanism of action between the two can be described, and then lays the first stone for the application of silicon ball aspect biological medicine.
Given this, the present invention adopts new assembling route, the outstanding advantage of fluorescent carbon quantum dot and porous silica material is combined, thereby prepare low toxicity, efficient, the stable controlled fluorescence SiO of pattern
2Nanometer ball, and will further explore its application on biological medicine carrying, thus use for it is following the gross data that provides necessary.
Summary of the invention
The preparation method who the purpose of this invention is to provide fluorescent silicon dioxide nanospheres that is to say that a kind of coated with silica fluorescent carbon quantum dot forms the preparation method of nano silicon spheres on every side.
The preparation method of a kind of fluorescent silicon dioxide nanospheres of the present invention is characterized in that having following process and step:
A. the preparation of the fluorescent carbon quantum dot of stearylamine modification
(1) preparation of fluorescent carbon quantum dot
By the prior art preparation, take a certain amount of disodium ethylene diamine tetraacetate (EDTA-2Na), put into quartz boat, and under nitrogen protection, calcined 2 hours under 250 ~ 400 ℃ in tube furnace, obtain fluorescent carbon quantum dot;
(2) modify fluorescent carbon quantum dot with stearylamine
Above-mentioned resulting a certain amount of fluorescent carbon quantum dot is dissolved in a certain amount of deionized water, carries out ultra-sonic dispersion, then carry out centrifugation, get its supernatant liquor; With acetic acid regulator solution pH value to 5 ~ 6, then add a certain amount of stearylamine and appropriate toluene in supernatant liquor, mix; Both weight ratios of the add-on of fluorescent carbon quantum dot and stearylamine are 1:1; Then, above-mentioned mixed solution is poured in reactor, reacted under 160 ~ 180 ℃ 12 ~ 14 hours; Then draw its upper strata liquid, oven dry under 60 ℃; Finally obtain the fluorescent carbon quantum dot that stearylamine is modified;
B. the preparation of (1) sub-aian fluorescent silicon dioxide nanospheres
(1) take the fluorescent carbon quantum dot that a certain amount of above-mentioned stearylamine that makes is modified, add a certain amount of deionized water, carry out ultra-sonic dispersion; After the fluorescent carbon quantum dot that described stearylamine is modified added water, the concentration of its solution was 0.005 ~ 0.01g/mL;
(2) get a certain amount of ethanol and add in mentioned solution, make to mix, then slowly add proper ammonia and tetraethoxy (TEOS) successively in solution; 40 ~ 50 ℃ of lower stirring reactions 1 ~ 12 hour; The add-on of ammoniacal liquor and tetraethoxy, both volume ratios are 1:(1 ~ 4);
(3) then, then in solution progressively slowly add tetraethoxy (TEOS) and cetyl trimethylammonium bromide (CTAB); The consumption of TEOS and CTAB recently measures by its volume weight, i.e. TEOS:CTAB=1:(0.35 ~ 0.5); That is to say the CTAB of every 1 mL TEOS adapted 0.35 ~ 0.5 g; Then slowly stirring reaction after 1 ~ 12 hour, is used the supercentrifuge centrifugation, gets its lower sediment;
(4) with above-mentioned precipitation with appropriate washing with alcohol after, layer precipitation taken off in then centrifugation, then repeatable operation 2 ~ 3 times is placed on described precipitation and continues oven dry 12 ~ 16 hours in 60 ℃ of baking ovens;
(5) then take out the product sample from baking oven, levigate with agate mortar, be placed on subsequently in tube furnace in 300 ℃ of calcinings 2 ~ 4 hours; Finally obtain fluorescent silicon dioxide nanospheres.
Now relevant mechanism and principle in the technological process of the inventive method are described below:
In technological process of the present invention, adopt ethanol as solvent, the carbon quantum dot that stearylamine is modified can access better dispersion; The effect of modifying fluorescent carbon quantum dot with stearylamine is to make the fluorescent carbon quantum dot surface amination, realizes that water changes to oil phase, singly is scattered in organic solvent.In step (2), add ammoniacal liquor mainly to play catalyzer, pH that can regulator solution is weakly alkaline, is conducive to the hydrolysis of TEOS in later step.The TEOS that step (2) and (3) add is fluorescence SiO
2The silicon source of nanometer ball, different is, and (2) step formed is kernel portion, was housing parts and (3) step formed.Add Surfactant CTAB mainly to play structure directing agent in step (3), be conducive to the formation of fluorescent silicon dioxide nanospheres novel texture.For the fluorescent carbon quantum dot that is not coated by SiO2 is cleaned up with ethanol repetitive scrubbing sample after reaction.
The characteristics of the inventive method products therefrom are the nucleocapsid structures of silicon bag carbon, are take fluorescent carbon quantum dot as core, the structure take silicon-dioxide as shell.
The fluorescent silicon dioxide nanospheres of gained of the present invention has that the high and low poison of chemical stability is even nontoxic, fluorescence is extremely stable, the emission wavelength wide region is adjustable, be easy to realize the characteristics such as physiologically acceptable; Through can be used for biological tissue's mark after the subsequent disposal such as finishing.Technique of the present invention is simple, and easy handling, cost are low.
Description of drawings
Fig. 1 is gained fluorescence SiO in the embodiment of the present invention 1
2The scanning electronic microscope of nanometer ball (SEM) photo;
Fig. 2 is gained fluorescence SiO in the embodiment of the present invention 1
2The fluorescence pattern of nanometer ball;
Fig. 3 is gained fluorescence SiO in the embodiment of the present invention 1
2The CONFOCOL photo of nanometer ball.
Embodiment
After now specific embodiments of the invention being described in.
Embodiment 1:
In the present embodiment, the preparation process of fluorescent silicon dioxide nanospheres is as follows:
1. the preparation of the fluorescent carbon quantum dot of stearylamine modification
(1) preparation of fluorescent carbon quantum dot
Prepare by published prior art, adopt the disodium ethylene diamine tetraacetate (EDTA-2Na) of 1.0 g, be placed in quartz boat, put under lower 380 ℃ of tube furnace nitrogen protection calcining 2 hours, obtain fluorescent carbon quantum dot;
(2) modify fluorescent carbon quantum dot with stearylamine
Get 0.5 g fluorescent carbon quantum dot and be dissolved in 30 mL water, ultra-sonic dispersion, its supernatant liquor 20 mL are got in then centrifugation, with the pH value to 5.5 of acetic acid regulator solution; Then add 0.5 g stearylamine and 20 mL toluene in supernatant liquor, mix; Then above-mentioned mixed solution is poured in reactor, reaction is 12 hours under 170 ℃; Then draw upper strata liquid, oven dry under 60 ℃; Finally obtain the fluorescent carbon quantum dot that stearylamine is modified;
2. the preparation of fluorescent silicon dioxide nanospheres
(1) take with electronic balance fluorescent carbon quantum dot 0.05 g that the above-mentioned stearylamine that makes is modified, add 8 mLH
2Ultra-sonic dispersion in O;
(2) graduated cylinder measures 40 mL ethanol (CH
3CH
2OH) add in solution and mix, then slowly add 1 mL ammoniacal liquor (NH successively in solution
4OH), 2 mL tetraethoxys (TEOS), 40 ℃ of lower stirring reactions 3 hours;
(3) progressively slowly add TEOS 2 mL in solution, cetyl trimethylammonium bromide (CTAB) 1.0 g, slowly stirring reaction is after 5 hours, with supercentrifuge centrifuging and taking lower sediment;
(4) precipitating with centrifuging and taking lower sediment after 25 mL washing with alcohol, repeatable operation 2 ~ 3 times.
(5) precipitation is placed on and continues oven dry 12 hours in 60 ℃ of baking ovens;
(6) take out sample in case levigate with agate mortar, be placed in tube furnace 300 ℃ of calcinings 2 hours.
Prepared sample is carried out physical property characterize, its partial results as shown in drawings.
Embodiment 2: the implementation process step except for the following differences, other are all identical with embodiment 1, difference is:
Graduated cylinder measures 40 mL ethanol (CH in (2) step
3CH
2OH) add in solution and mix, then slowly add 1 mL ammoniacal liquor (NH successively in solution
4OH), 1 mL tetraethoxy (TEOS), during 40 ℃ of lower stirring reactions 1;
Progressively slowly add TEOS 1 mL, cetyl trimethylammonium bromide (CTAB) 0.5 g in (3) step in solution, slowly stirring reaction is after 1 hour, with supercentrifuge centrifuging and taking lower sediment.Result is substantially similar to embodiment 1, and difference is fluorescence SiO
2The housing parts of nanometer ball is slightly thinner on thickness than embodiment 1.
Embodiment 3: the implementation process step except for the following differences, other are all identical with embodiment 1, difference is:
In (2) step, measure 40 mL ethanol (CH with graduated cylinder
3CH
2OH) add in solution and mix, then slowly add 1 mL ammoniacal liquor (NH successively in solution
4OH), 4 mL tetraethoxys (TEOS), 40 ℃ of lower stirring reaction 12 h;
In (3) step, progressively slowly add TEOS 4 mL, cetyl trimethylammonium bromide (CTAB) 1.5 g in solution, slowly stirring reaction is after 12 hours, with supercentrifuge centrifuging and taking lower sediment;
Result is similar to embodiment 1, and difference is fluorescence SiO
2The kernel portion of nanometer ball and housing parts are all slightly thick on thickness than embodiment 1, and fluorescence property slightly weakens.
Instrument detects
Embodiment 1 products therefrom is made every instrument detect, detected result is shown in accompanying drawing Fig. 1, Fig. 2 and Fig. 3, and referring to accompanying drawing, Fig. 1 is gained fluorescence SiO in the embodiment of the present invention 1
2The SEM photo of nanometer ball.Sem analysis: adopt Japanese Hitachi S-4800 type sem observation material surface pattern and size-grade distribution.Therefrom can find out: gained fluorescence silicon composite is spherical nanoparticle, and particle diameter is evenly distributed about 80 nm, the pattern homogeneous.
Referring to accompanying drawing, Fig. 2 is gained fluorescence SiO in the embodiment of the present invention 1
2The fluorescence pattern of nanometer ball.Fluorometric analysis: the F-7000 type spectrophotofluorometer detection fluorescence SiO that adopts HITACHI company
2The fluorescence intensity of nanometer ball.Therefrom as can be known, the fluorescence SiO that makes
2Nanometer ball is at 700V voltage, and 320 nm wavelength excite good diffraction peak intensity about 400 nm.
Referring to accompanying drawing, Fig. 3 is gained fluorescence SiO in the embodiment of the present invention 1
2The Confocol photo of nanometer ball.Confocol analyzes: adopt the FV1000 type confocal microscope of Olympus company at the 488 nm wavelength excitation-detection fluorescence SiO of place
2The fluorescence intensity of nanometer ball and particle distribution situation.Therefrom as can be known, gained SiO
2Nanometer ball particle monodispersity is good, sends blue fluorescence.
Claims (1)
1. the preparation method of a fluorescent silicon dioxide nanospheres is characterized in that having following preparation process and step:
A. the preparation of the fluorescent carbon quantum dot of stearylamine modification
(1) preparation of fluorescent carbon quantum dot
By the prior art preparation, adopt a certain amount of disodium ethylene diamine tetraacetate (EDTA-2Na) to put into quartz boat, and under nitrogen protection, calcined 2 hours under 250 ~ 400 ℃ in tube furnace, obtain fluorescent carbon quantum dot;
(2) modify fluorescent carbon quantum dot with stearylamine
Above-mentioned resulting a certain amount of fluorescent carbon quantum dot is dissolved in a certain amount of deionized water, carries out ultra-sonic dispersion, then carry out centrifugation, get its supernatant liquor; With acetic acid regulator solution pH value to 5 ~ 6, then add a certain amount of stearylamine and appropriate toluene in supernatant liquor, mix; Both weight ratios of the add-on of fluorescent carbon quantum dot and stearylamine are 1:1; Then, above-mentioned mixed solution is poured in reactor, reacted under 160 ~ 180 ℃ 12 ~ 14 hours; Then draw its upper strata liquid, oven dry under 60 ℃; Finally obtain the fluorescent carbon quantum dot that stearylamine is modified;
B. the preparation of fluorescent silicon dioxide nanospheres
(1) take the fluorescent carbon quantum dot that a certain amount of above-mentioned stearylamine that makes is modified, add a certain amount of deionized water, carry out ultra-sonic dispersion; After the fluorescent carbon quantum dot that described stearylamine is modified added water, the concentration of its solution was 0.005 ~ 0.01 g/mL;
(2) get a certain amount of ethanol and add in mentioned solution, make to mix, then slowly add proper ammonia and tetraethoxy (TEOS) successively in solution; 40 ~ 50 ℃ of lower stirring reactions 1 ~ 12 hour; The add-on of ammoniacal liquor and tetraethoxy, both volume ratios are 1:(1 ~ 4);
(3) then, then in solution progressively slowly add tetraethoxy (TEOS) and cetyl trimethylammonium bromide (CTAB); The consumption of TEOS and CTAB recently measures by its volume weight, i.e. TEOS:CTAB=1:(0.35 ~ 0.5); That is to say the CTAB of every 1 mL TEOS adapted 0.35 ~ 0.5 g; Then slowly stirring reaction after 1 ~ 12 hour, is used the supercentrifuge centrifugation, gets its lower sediment;
(4) with above-mentioned precipitation with appropriate washing with alcohol after, layer precipitation taken off in then centrifugation, then repeatable operation 2 ~ 3 times is placed on described precipitation and continues oven dry 12 ~ 16 hours in 60 ℃ of baking ovens;
(5) then take out the product sample from baking oven, levigate with agate mortar, be placed on subsequently in tube furnace in 300 ℃ of calcinings 2 ~ 4 hours; Finally obtain fluorescent silicon dioxide nanospheres.
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